CN102569736B - Carbon-coated graphene oxide composite material as well as preparation method and application thereof - Google Patents
Carbon-coated graphene oxide composite material as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a carbon-coated graphene oxide composite material as well as a preparation method and an application of the carbon-coated graphene oxide composite material. The carbon-coated graphene oxide composite material comprises the following steps of: obtaining graphene oxide; mixing the graphene oxide with an organic carbon source according to a mass percent of (1-10):1 to form a mixture; and pyrolyzing and cooling the mixture in oxygen-free environment, and obtaining the carbon-coated graphene oxide composite material. The preparation method of the carbon-coated graphene oxide composite material has the advantages that the process is simple, the energy consumption is small, the cost is low, the pollution is avoided, and the preparation method is suitable for industrial production. The carbon-coated graphene oxide composite material prepared by the method has the advantages that the structure performance is stable, the electrical conductivity is high, and the power density is high when the carbon-coated graphene oxide composite material is used for preparing cathode materials in lithium ion batteries or/and capacitors.
Description
Technical field
The invention belongs to technical field of inorganic chemical industry, relate to coated graphene oxide composite material of a kind of carbon and preparation method thereof and application specifically.
Background technology
Since strong K sea nurse (Andre K.Geim) of peace moral etc. of Univ Manchester UK prepared grapheme material in 2004.Pay attention to widely because the structure of its uniqueness and photoelectric property receive people.Mono-layer graphite due to its large specific area, excellent conduction, heat conductivility and low thermal coefficient of expansion and be considered to desirable material.As: 1, high strength, Young mole, (1,100GPa), fracture strength: (125GPa); 2, high heat conductance, (5,000W/mK); 3, high conductivity, carrier transport rate, (200,000cm
2/ V*s); 4, high specific area, (calculated value: 2,630m
2/ g).Especially the structural property of the nanoscale of its high connductivity character, large specific surface character and its monolayer two dimension, can be widely used in electrode material.In addition, Yang Quanhong etc. are under vacuum degree 0.01Pa ~ 10kPa, graphite oxide is warmed up to 150 ~ 600 DEG C with the heating rate of 5 ~ 50 DEG C/min and carries out hypertonic solutions, maintain constant temperature 0.5 ~ 20h, graphite oxide rapid spatial expansion, obtain specific area 200 ~ 800m2/g, the graphene oxide composite material of electrochemical specific capacity 50 ~ 200F/g.Generally speaking, due to containing-C-OH ,-C-O-C in graphene oxide, the even group such as-COOH, thus show stronger polarity.The dry aerial less stable of graphene oxide, is easy to the moisture absorption and forms aquation graphene oxide.As electrode material, graphene oxide has discharge capacity and good with electrolyte wettability, but graphene oxide also comes with some shortcomings, as relatively low in fluorinated graphite rate, stability need further raising, thus causes the poor grade of battery high-rate performance not enough.
Summary of the invention
The object of the embodiment of the present invention is the above-mentioned deficiency overcoming prior art, provides that a kind of technique is simple, energy consumption is little, with low cost, is applicable to coated graphene oxide composite material of carbon of suitability for industrialized production and preparation method thereof.
And, the coated graphene oxide composite material of above-mentioned carbon as lithium ion battery or/and the application of positive electrode in capacitor.
In order to realize foregoing invention object, technical scheme of the present invention is as follows:
The coated graphene oxide composite material preparation method of a kind of carbon, comprises the steps:
Obtain graphene oxide;
Described graphene oxide and organic carbon source to be mixed by mass percentage at 1 ~ 10: 1, forms mixture;
Described mixture is carried out pyrolysis in oxygen-free environment, and cooling, obtains the coated graphene oxide composite material of described carbon.
And the coated graphene oxide composite material of a kind of carbon, the coated graphene oxide composite material of this carbon is prepared from by said method.
Further, the coated graphene oxide composite material of the carbon of the embodiment of the present invention as lithium ion battery or/and the application of positive electrode in capacitor.
Above-mentioned carbon coated graphene oxide composite material preparation method graphene oxide is mixed with organic carbon source carry out pyrolysis product, its preparation method technique is simple, energy consumption is little, with low cost, pollution-free, be applicable to suitability for industrialized production.Be combined with graphene oxide by carbon in the coated graphene oxide composite material prepared by the method, form the rock-steady structure of the coated graphene oxide of carbon, impart the high conductivity performance of the coated graphene oxide composite material of carbon and large power density.Use it for and prepare lithium ion battery or/and in capacitor during positive electrode, lithium ion battery is or/and capacitor power density is large.
Accompanying drawing explanation
Fig. 1 is carbon of the present invention coated graphene oxide composite material preparation method process flow diagram;
Fig. 2 is the XRD collection of illustrative plates of the coated graphene oxide composite material of carbon that the embodiment of the present invention 1 obtains;
Fig. 3 is the ultracapacitor containing the positive plate utilizing the obtained coated graphene oxide composite material of carbon of the embodiment of the present invention 1 to prepare is 0 ~ 2.0V in voltage range, and electric current is charge and discharge curve chart first under the condition of 1A/g.
Embodiment
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Example of the present invention provides that a kind of technique is simple, energy consumption is little, with low cost, be applicable to the coated graphene oxide composite material preparation method of carbon of suitability for industrialized production.This carbon coated graphene oxide composite material preparation method technological process refers to Fig. 1, and the method comprises the steps:
S1: obtain graphene oxide;
S2: graphene oxide and organic carbon source to be mixed by mass percentage at 1 ~ 10: 1, forms mixture;
S3: mixture is carried out pyrolysis in oxygen-free environment, cooling, obtains the coated graphene oxide composite material of carbon.
Particularly, in the S1 step of the coated graphene oxide composite material preparation method of above-mentioned carbon, graphene oxide acquisition methods refers to embodiment 1.
In the S2 step of the coated graphene oxide composite material preparation method of above-mentioned carbon, the mass ratio of graphene oxide and organic carbon source is preferably 2 ~ 5: 1.Wherein, organic carbon source is preferably at least one in sucrose, glucose, polyethylene glycol.The existence of the carbon source of this content and kind, being carbonized of pyrolysis in following S3 step, for the coated graphene oxide composite material of embodiment of the present invention carbon provides appropriate carbon source, make the coated graphene oxide composite material Stability Analysis of Structures of this carbon, conductance is high.
Further, in this S2 step, when organic carbon source is solid, as during for sucrose, in mixture, is also added with solvent, and heats, form pasty mixture.Wherein, solvent is preferably at least one in water, ethanol, acetone.The temperature of heating is preferably 60 ~ 100 DEG C, and the time is preferably 8 ~ 15h.In heating process, preferably stir simultaneously, each component is mixed, thus forms homogeneous pasty mixture.
In the S3 step of the coated graphene oxide composite material preparation method of above-mentioned carbon, the temperature of pyrolysis is preferably 300 ~ 600 DEG C, more preferably 500 DEG C; Time is preferably 3 ~ 10h, more preferably 8h.Mixture is preferably put into tube furnace and is carried out pyrolysis by this pyrolysis.This preferred pyrolytical condition more can be conducive to the carbonization of organic carbon source.Oxygen-free environment is the oxygen-free environment being full of nitrogen, other inert gases can certainly be adopted to substitute nitrogen, as Ar gas etc., vacuum also can be adopted to realize oxygen-free environment.
Above-mentioned carbon coated graphene oxide composite material preparation method graphene oxide is mixed with organic carbon source carry out pyrolysis product, its preparation method technique is simple, energy consumption is little, with low cost, pollution-free, be applicable to suitability for industrialized production.
The embodiment of the present invention additionally provides the coated graphene oxide composite material of a kind of carbon, is obtained by said method.The coated graphene oxide composite material of this carbon is combined with graphene oxide by carbon, forms the rock-steady structure of the coated graphene oxide of carbon, imparts the high conductivity performance of the coated graphene oxide composite material of carbon and large power density.Wherein, in the coated graphene oxide composite material of carbon, the mass fraction of the carbon of coated graphene oxide is 10% ~ 50%.
Have above-mentioned premium properties just because of the coated graphene oxide composite material of above-mentioned carbon, therefore, the embodiment of the present invention additionally provides the coated graphene oxide composite material of above-mentioned carbon as lithium ion battery further or/and the application of positive electrode in capacitor.By coated for this carbon graphene oxide composite material for the preparation of lithium ion battery or/and positive electrode in capacitor time, lithium ion battery is or/and capacitor power density is large.
Below by way of multiple embodiment difference composition illustrating the coated graphene oxide composite material of carbon and preparation method thereof, and the aspect such as its performance.
Embodiment 1
The preparation method of the coated graphene oxide composite material of carbon, its method technological process is as follows:
Coated graphene oxide → the Performance Detection of graphite → graphite oxide → carbon
S1: obtain graphene oxide;
S2: graphene oxide and organic carbon source to be mixed by mass percentage at 1 ~ 10: 1, forms mixture;
S3: mixture is carried out pyrolysis in oxygen-free environment, cooling, obtains the coated graphene oxide composite material of carbon.
S11. graphite oxide: by improve Hummers legal system for graphene oxide, its concrete steps are: by the graphite powder (50 order) of 20g purity 99.5%, the potassium peroxydisulfate of 10g and the phosphorus pentoxide of 10g join in the concentrated sulfuric acid of 80 DEG C, stir, cooling more than 6h, refilter, washing is to neutral, dry, and dried sample is added 0 DEG C, in the concentrated sulfuric acid of 230ml, then 60g potassium permanganate is added, and temperature is remained on less than 20 DEG C, then after keeping 2h in the oil bath of 35 DEG C, slowly add 920ml deionized water, after 15min, continue to add 2.8L deionized water (wherein containing 50ml concentration is the hydrogen peroxide of 30%), mixture color becomes glassy yellow afterwards, suction filtration while hot, finally wash with the hydrochloric acid that 5L concentration is 10%, suction filtration, namely graphene oxide is obtained at 60 DEG C of vacuumize 48h,
S12. the coated graphene oxide of carbon: get graphite oxide 10g prepared by S11 step, adds water and 5g sucrose wherein, stirs and graphite oxide and sucrose are mixed, and then heating makes mixture become pasty state;
S13. pasty mixture is placed in 300 DEG C of insulation 10h under the condition that tube furnace protects at nitrogen atmosphere, after naturally cooling, obtains the coated graphene oxide composite material of carbon.
The coated graphene oxide composite material of the carbon prepared by the present embodiment carries out X-ray diffraction analysis, obtains the XRD collection of illustrative plates of the coated graphene oxide composite material of this carbon, as shown in Figure 2.Occurring the diffraction maximum of graphene oxide as seen from Figure 2 at about 11 DEG C, have no the diffraction maximum of carbon, may be carbon for amorphous state or the less reason of content.
The coated graphene oxide composite material of the carbon prepared by the present embodiment is used for the preparation of positive plate, and preparation method is as follows:
The preparation of pole piece: take the coated graphene oxide composite material 4.5g of carbon, acetylene black 0.25g, PVDF0.25g, dripping NMP makes said mixture become pulpous state, be coated on metal aluminum foil after abundant stirring makes it to mix, coating thickness is 200 μm, then take out after vacuum 100 DEG C of dry 12h, form described pole piece;
Pole piece roll-in: pole piece roller mill is carried out roll extrusion, the thickness after roll-in is 165 μm;
Cut-parts: the pole piece card punch of roll-in is broken into the circular pole piece that diameter is 10mm, correct amount;
The assembling of ultracapacitor: by pole piece in glove box, barrier film and electrolyte are assembled into ultracapacitor according to cell making process, its septation is the 1-ethyl-3-methylimidazole tetrafluoro boric acid salting liquid of celgard2000,0.5mol/L is electrolyte, has assembled latter standing one day.
Performance Detection: ultracapacitor positive plate being prepared by the coated graphene oxide composite material of carbon obtained containing the present embodiment 1 is 0 ~ 2.0V in voltage range, electric current is carry out constant current charge-discharge after tested under the condition of 1A/g, this ultracapacitor charge and discharge specific capacity and efficiency for charge-discharge test result are in table 1, it is 0 ~ 2.0V in voltage range, electric current be under the condition of 1A/g first charge and discharge curve chart as Fig. 3.From table 1 and Fig. 3, large containing utilizing the coated graphene oxide composite material of carbon to prepare the ultracapacitor power density of positive plate, current constant, its charge specific capacity is 115.01F/g, specific discharge capacity is 107.59F/g, efficiency for charge-discharge, up to 93.54%, illustrates that the present embodiment carbon coated graphene oxide composite material high rate performance is better.
Embodiment 2
The preparation of the coated graphene oxide composite material of carbon, its method technological process is as follows:
S21. graphite oxide: see the S11 step in embodiment 1;
S22. the preparation of the coated graphene oxide composite material of carbon: get graphite oxide 20g prepared by S21 step, adds water and 5g sucrose wherein, stirs and graphite oxide and sucrose are mixed, and then heating makes mixture become pasty state;
S23. pasty mixture is placed in 500 DEG C of insulation 5h under the condition that tube furnace protects at nitrogen atmosphere, cooling, obtains carbon coated graphene oxide composite material naturally.
The coated graphene oxide composite material of the carbon obtained by the present embodiment is used for the preparation of positive plate.The steps such as this positive plate preparation method comprises the preparation of pole piece, roll-in, cut-parts, the assembling of its concrete preparation process and the ultracapacitor containing this positive plate refer to embodiment 1.This ultracapacitor is 0 ~ 2.0V in voltage range, and electric current is carry out constant current charge and discharge after tested under the condition of 1A/g, and this ultracapacitor charge and discharge specific capacity and efficiency for charge-discharge test result are in table 1.
Embodiment 3
The preparation of the coated graphene oxide composite material of carbon, its method technological process is as follows:
S31. graphite oxide: see the S11 step in embodiment 1;
S32. the preparation of the coated graphene oxide composite material of carbon: get graphite oxide 20g prepared by S31 step, adds water and 5g sucrose wherein, stirs and graphite oxide and sucrose are mixed, and then heating makes mixture become pasty state;
S33. pasty mixture is placed in 600 DEG C of insulation 3h under the condition that tube furnace protects at nitrogen atmosphere, cooling, obtains carbon coated graphene oxide composite material naturally.
The coated graphene oxide composite material of the carbon obtained by the present embodiment is used for the preparation of positive plate.The steps such as this positive plate preparation method comprises the preparation of pole piece, roll-in, cut-parts, the assembling of its concrete preparation process and the ultracapacitor containing this positive plate refer to embodiment 1.This ultracapacitor is 0 ~ 2.0V in voltage range, and electric current is carry out constant current charge and discharge after tested under the condition of 1A/g, and this ultracapacitor charge and discharge specific capacity and efficiency for charge-discharge test result are in table 1.
Embodiment 4
The preparation of the coated graphene oxide composite material of carbon, its method technological process is as follows:
S41: graphite oxide: see the S11 step in embodiment 1;
S42: the preparation of the coated graphene oxide composite material of carbon: get graphite oxide 20g prepared by S41 step, adds water and 5g polyethylene glycol wherein, stirs and graphite oxide and sucrose are mixed, and then heating makes mixture become pasty state;
S43. pasty mixture is placed in 500 DEG C of insulation 5h under the condition that tube furnace protects at nitrogen atmosphere, cooling, obtains carbon coated graphene oxide composite material naturally.
The coated graphene oxide composite material of the carbon obtained by the present embodiment is used for the preparation of positive plate.The steps such as this positive plate preparation method comprises the preparation of pole piece, roll-in, cut-parts, the assembling of its concrete preparation process and the ultracapacitor containing this positive plate refer to embodiment 1.This ultracapacitor is 0 ~ 2.0V in voltage range, and electric current is carry out constant current charge and discharge after tested under the condition of 1A/g, and this ultracapacitor charge and discharge specific capacity and efficiency for charge-discharge test result are in table 1.
Embodiment 5
The preparation of the coated graphene oxide composite material of carbon, its method technological process is as follows:
S51: graphite oxide: see the S11 step in embodiment 1;
S52: the preparation of the coated graphene oxide composite material of carbon: get graphite oxide 20g prepared by S51 step, add sucrose and polyethylene glycol mixture that water and 2g mass ratio are 1: 1 wherein, stirring makes graphite oxide, sucrose, polyethylene glycol mix, and then heating makes mixture become pasty state;
S53. pasty mixture is placed in 400 DEG C of insulation 10h under the condition that tube furnace protects at nitrogen atmosphere, cooling, obtains carbon coated graphene oxide composite material naturally.
The coated graphene oxide composite material of the carbon obtained by the present embodiment is used for the preparation of positive plate.The steps such as this positive plate preparation method comprises the preparation of pole piece, roll-in, cut-parts, the assembling of its concrete preparation process and the ultracapacitor containing this positive plate refer to embodiment 1.This ultracapacitor is 0 ~ 2.0V in voltage range, and electric current is carry out constant current charge and discharge after tested under the condition of 1A/g, and this ultracapacitor charge and discharge specific capacity and efficiency for charge-discharge test result are in table 1.
Embodiment 6
The preparation of the coated graphene oxide composite material of carbon, its method technological process is as follows:
S61: graphite oxide: see the S11 step in embodiment 1;
S62: the preparation of the coated graphene oxide composite material of carbon: get graphite oxide 20g prepared by S61 step, adds water and 1g sucrose wherein, stirs and graphite oxide and sucrose are mixed, and then heating makes mixture become pasty state;
S63. pasty mixture is placed in 300 DEG C of insulation 4h under the condition that tube furnace protects at nitrogen atmosphere, cooling, obtains carbon coated graphene oxide composite material naturally.
The coated graphene oxide composite material of the carbon obtained by the present embodiment is used for the preparation of positive plate.The steps such as this positive plate preparation method comprises the preparation of pole piece, roll-in, cut-parts, the assembling of its concrete preparation process and the ultracapacitor containing this positive plate refer to embodiment 1.This ultracapacitor is 0 ~ 2.0V in voltage range, and electric current is carry out constant current charge and discharge after tested under the condition of 1A/g, and this ultracapacitor charge and discharge specific capacity and efficiency for charge-discharge test result are in table 1.
Embodiment 7
The preparation of the coated graphene oxide composite material of carbon, its method technological process is as follows:
S71: graphite oxide: see the S11 step in embodiment 1;
S72: the preparation of the coated graphene oxide composite material of carbon: get graphite oxide 20g prepared by S71 step, add sucrose and polyethylene glycol mixture that water and 20g mass ratio are 1: 4 wherein, stirring makes graphite oxide, sucrose and polyethylene glycol mix, and then heating makes mixture become pasty state;
S73. pasty mixture is placed in 500 DEG C of insulation 8h under the condition that tube furnace protects at nitrogen atmosphere, cooling, obtains carbon coated graphene oxide composite material naturally.
The coated graphene oxide composite material of the carbon obtained by the present embodiment is used for the preparation of positive plate.The steps such as this positive plate preparation method comprises the preparation of pole piece, roll-in, cut-parts, the assembling of its concrete preparation process and the ultracapacitor containing this positive plate refer to embodiment 1.This ultracapacitor is 0 ~ 2.0V in voltage range, and electric current is carry out constant current charge and discharge after tested under the condition of 1A/g, and this ultracapacitor charge and discharge specific capacity and efficiency for charge-discharge test result are in table 1.
Embodiment 8
The preparation of the coated graphene oxide composite material of carbon, its method technological process is as follows:
S81: graphite oxide: see the S11 step in embodiment 1;
S82: the preparation of the coated graphene oxide composite material of carbon: get graphite oxide 20g prepared by S81 step, adds water and 10g glucose wherein, stirs and graphite oxide and glucose are mixed, and then heating makes mixture become pasty state;
S83. pasty mixture is placed in 500 DEG C of insulation 6h under the condition that tube furnace protects at nitrogen atmosphere, cooling, obtains carbon coated graphene oxide composite material naturally.
The coated graphene oxide composite material of the carbon obtained by the present embodiment is used for the preparation of positive plate.The steps such as this positive plate preparation method comprises the preparation of pole piece, roll-in, cut-parts, the assembling of its concrete preparation process and the ultracapacitor containing this positive plate refer to embodiment 1.This ultracapacitor is 0 ~ 2.0V in voltage range, and electric current is carry out constant current charge and discharge after tested under the condition of 1A/g, and this ultracapacitor charge and discharge specific capacity and efficiency for charge-discharge test result are in table 1.
Table 1 ultracapacitor charge and discharge specific capacity and efficiency for charge-discharge
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. the coated graphene oxide composite material preparation method of carbon, comprises the steps:
Obtain graphene oxide;
By described graphene oxide and organic carbon source by mass percentage 2 ~ 10:1 mix, form mixture; Wherein, when organic carbon source is solid, in mixture, also add solvent, and in 60-100 DEG C of heating 8-15h, form pasty mixture; Described organic carbon source is at least one in sucrose, glucose organic substance;
Described mixture is carried out pyrolysis in oxygen-free environment, and cooling, obtain the coated graphene oxide composite material of described carbon, in the coated graphene oxide composite material of described carbon, the mass fraction of the carbon of coated graphene oxide is 10% ~ 50%.
2. the coated graphene oxide composite material preparation method of carbon according to claim 1, is characterized in that: the mass ratio of described graphene oxide and organic carbon source is 2 ~ 5:1.
3. the coated graphene oxide composite material preparation method of carbon according to claim 1, is characterized in that: the temperature of described pyrolysis is 200 ~ 800 DEG C, and the time is 1 ~ 12h.
4. the coated graphene oxide composite material preparation method of carbon according to claim 3, is characterized in that: the temperature of described pyrolysis is 300 ~ 600 DEG C, and the time is 3 ~ 10h.
5. the coated graphene oxide composite material preparation method of carbon according to claim 4, is characterized in that: the temperature of described pyrolysis is 500 DEG C, and the time is 8h.
6. the coated graphene oxide composite material of carbon, is characterized in that: the coated graphene oxide composite material of described carbon obtains according to the arbitrary described coated graphene oxide composite material preparation method of carbon of Claims 1 to 5.
7. the coated graphene oxide composite material of carbon according to claim 6 as lithium ion battery or/and the application of positive electrode in capacitor.
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| CN102969508A (en) * | 2012-12-06 | 2013-03-13 | 苏州大学 | Preparation method and application of carbon-coated graphene composite material for lithium ion battery |
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| CN104064366A (en) * | 2013-03-18 | 2014-09-24 | 海洋王照明科技股份有限公司 | Graphene-hard carbon composite material, preparation method thereof and application thereof |
| CN103626151A (en) * | 2013-11-28 | 2014-03-12 | 复旦大学 | Preparation method of graphene/carbon composite material |
| CN104377346B (en) * | 2014-11-04 | 2017-05-03 | 辽宁工程技术大学 | Method for preparing modified graphite negative electrode material of sodium ion battery |
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| CN107331845B (en) * | 2017-07-05 | 2020-01-14 | 湖南泰和美新能源科技有限公司 | Graphene battery positive electrode composite material |
| CN107507967B (en) * | 2017-07-13 | 2020-10-09 | 贵州鼎玺烯材高科技有限公司 | Graphene battery cathode composite material |
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